Recovery of hydrocarbons and acetone from admixtures by phase separation and azeotropic distillation



July 8 1947- J. A. PATTERSON 2,423,795

' RECOVERY 0F HYDROCARBONS AND ACETONE FROM ADMIXTURES BY PHASE SEPARATION AND ZEOTROPIC DISTILLATION Filed Jan. 1, 194s NIX TGR E @atented .Furty d? masses John a. Patterson, Westfield, N. r., assigner to Standard i! Development Company, a corporation of Delaware Application January 1, 1943, serial Namaste d Claims.

This invention relates to the treatment of hydrocarbon solutions containing acetone, in order to eiect separation of the constituents in a commercially advantageous mannen The invention relates particularly to the separation of the hyrecovered in a highly purified state by passing drocarbon and acetone from the products of exthe upper essentially hydrocarbon layer to a distractive distillation systems. tillation system and adding such quantities of Many processes are at present being employed water as are required to form an -azectropic for the separation of valuable hydrocarbons from ternary composition of hydrocarbon, acetone and complex mixtures, such as refinery by-products, water with all of the acetone present in the hyfor the preparation of chemical specialties and drocarbon ph'ase. Thus, all the acetone is dissynthetic products. One particularly advantatilled from the hydrocarbon as` its ternary geous manner of processing complex hydrocarazeotropic mixture with the hydrocarbon and wabon mixtures to separate the relatively volatile ter, having as the distillation residue the hydrolow n'iolecular-weightI unsaturated hydrocarbons 15 carbon free of solvent and water. The azeotropic is the combination of fractional distillation and mixture will clearly contain a considerably higher extractive distillation. In extractive distillation concentration of the solvent and lower concen-v the solvents employed are frequently water solutration of the hydrocarbon than the hydrocarble and quite commonly admixed with water, and bon phase initially fed to the distillation tower. form azeotropic mixtures with the hydrocarbon The azeotropi'c distillate may be treated in a products. The commercial advantage of such manner similar to that to which the product processing increases as the degree of recovery of from the extractive distillation Was subjected. the solvent employed inthe extractive distillation In this manner all of the hydrocarbon maybe is made more efficient. When the solvent emrecovered in a highly purified state while all of ployed in an extractive distillation is water soluthe solvent is recovered as its solution in water. ble, the method of removing the solvent from the Clearly also, an added advantage in such processproducts of the extractiva distillation system may ing is the addition to the upper essentially hydroclearly be effected by water treatment. Such carbon layer in the distillation operation of contreatment however has in general the disadtrolledamountsofthe substantially aqueous phase vantages of requiring relatively large volumes of rather than of water. The present invention is water and thus the production of very dilute the commercial utilization of such treatments as solutions which are costly to distill for the rer the means for separating the hydrocarbon and covery of the primary solvent. solvent materials from the distillate products of It is an object of the present invention to proextractive distillation systems employing Watervide a cheaper and more eiilcient means of` resoluble acetone. covering acetone from the products of an ex- Thus, the invention relates particularly to the tractive distillation system in which acetone is distillate products of extractive distillation sysemployed. It is also an object of the invention tems treating complex hydrocarbon mixtures emto furnish processing for the separation of inploying acetone. The methodisto add an amount dividual hydrocarbons from complex mixtures 40 of water to the mixture of acetone and hydroupon g. particularly advantageous economic basis carbon suilicient to cause a, separation of a diby utilizing the formation of azeotropic composiphase ternary mixture. After phase separation tions/which commonly occur in many extractive the upper or essentially hydrocarbon phase is redistillation systems employing acetone as a means moved and distilled inthe presence of just enough of recovering the solvents themselves. Oth'er ob- 45 water or of the lower or aqueous phase to effect jects will be apparent from the reading of the i the separation as a distillate material a. ternary following description of the invention. y azeotropic composition of hydrocarbon, acetone If water be added to the distillate products of and water. The amount of water added to the an extractive distillation system in which a comdistillation system is adjusted to hold the quanplex hydrocarbon mixture is being treated and in tity of aqueous phase thus reuxed in the preferwhich acetone is being employed, a diphase able means of operation to a, practical minimum. ternary liquid mixture can be formed. In the On condensation, the ternary azeotrope may be phase separation o! such a mixture, the upper made to separate into two layers suitable for conphase consists predominantly of hydrocarbons. a tinued processions by the addition of controlled vminor quantity of acetone and a lesser amount quantity of hydrocarbon material. From such a diphase mixture the hydrocarbon'material can be amounts of water. Each of these phases may be carbon. The amount of aqueous or lower layer f not supplied to the azeotropic distillation column is subjected to 'a simple distillation, and thus there is obtained as products from this operation relatively pure solvent and essentially solventfree water. The solvent-water mixture however supplied as feed to this distillation treatment is much richer than that obtained by solvent extraction processing with Water of the spent hydrocarlbon fraction from-the extractive distillation system. Thus, a considerable saving in operating costs is effected.

In order to illustrate more specifically the invention, the following example of one method of operating according to the invention is presented. In the description, reference is made to solvent recovery after extractive distillation with acetone as the solvent of a mixture of C5 hydrocarbons. The numerals given in the description refer to the accompanying drawing.

A mixture of Cs hydrocarbons and acetone condensed from the overhead vapors leaving a vaporliquid extraction zone, which may contain from 4 to 12% acetone, is shown as stream I entering a decanter, 3. Also entering the decanter through line 8 isa two-phase condensed mixture of acetone, water, and hydrocarbon and a stream of water through line 2 limited in amount in accordance with the previous analysis of the invention. In the present instance, it will be about 10% base on the feed for` 10% acetone in the feed. The mixture in the decanter separates into two layers, the upper layer being fed through line 4 to the top of the azeotropic distillation column 5, and the lower layer being fed through line I to -a suitable intermediate point of the solvent recovery column I2. Steam is supplied to a heating coil, 9 in the first column, and is blown directly into the bottom of the second column through line I9. The overhead fraction leaving the first distillation column through line 6 is condensed in condenser 1 and mixed with the feed to the decanter'as mentioned previously, while the bottoms from the column leaving through line I I consist essentially of solvent-free C hydrocarbon, which may be utilized in any desired manner.

The overhead fraction leaving the second, or solvent recovery column through line I3 is condensed in equipment I4 and allowed to run through line I5 into the drum I6. From the drum IS part of the condensa-te is returned to the top of the column as reilux through line I1 while the vent-free water, and may be discarded or partially returned to the decanter through line 2.

Thus, processing according to the invention involves not only a saving in processing costs due 'to the handling of a more concentrated acetone stream, but .also the advantage of there being a much rless increase in investment cost than is necessitated Iby the us'e of an additional distillation column, when 'solvent extraction methods for recovery of the solvent m'aterial are employed. The saving is made Iby reason of the fact that the diameter and number of plates in the solvent l recovery column are substantially reduced.

What is claimed is: 1. The method of recovering aliphatic hydroearbons and acetone from a. distillate productor an extractive distillation system employing aceremainder is withdrawn through line I8 as recovered solvent. rI'his latter quantity of recovered solvent may be recycled to the vapor-liquid extraction zone.` The bottoms leaving the second column through line 20 consist of essentially soltone as the solvent in the treatment of a complex hydrocarbon mixture, .which comprises adding Water tothe said distillate product to effect a.

diphase separation of an essentially hydrocarbon phase and an essentially aqueous acetone phase, distilling the essentially hydrocarbon phase with water i'n/an amount to form a ternary azeotropic composition with the hydrocarbons and all of the acetone present, and recovering the hydrocarbons and the acetone from the products thus formed.

2. The method according `to claim 1 in which the amount of water to form with the essentially hydrocarbon phase upon distillation of the said ternary azeotropic composition` is supplied by the addition of a suitable quantity of the essentially aqueous'acetone .phase formed from the said distillate product of the said extractive distillation system.

3. The method according to claim 1 in which the ternary azeotropic composition is combined with the distillate product from the extractive distillation. f

4. The method according to claim 1 in which the ternary azeotropic composition is diphase and in which the recovery of the hydrocarbon and solvent materials is aided by combining separately the two essentially hydrocarbon phases respectjvely and the two essentially aqueous solvent phases respectively.

. JOHN A. PATTERSON.

REFERENCES lCITED The following references are of record in the ille of this patent:

UNITED STATES PATENTS I Austria Oct. 26, 1925 

